CN1580190A - Method for preparing biodiesel by solid acid-base catalyst - Google Patents
Method for preparing biodiesel by solid acid-base catalyst Download PDFInfo
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- CN1580190A CN1580190A CNA2004100382924A CN200410038292A CN1580190A CN 1580190 A CN1580190 A CN 1580190A CN A2004100382924 A CNA2004100382924 A CN A2004100382924A CN 200410038292 A CN200410038292 A CN 200410038292A CN 1580190 A CN1580190 A CN 1580190A
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- oil
- bio
- solid acid
- solid
- diesel oil
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
Abstract
The invention relates a kind of preparation method of bio-diesel oil under the condition of solid ac and alk catalyzing. The character is that under the condition of solid ac and alk catalyzing, gain the bio-diesel oil using the craft of exchange reaction of soja oil with carbinol. Afer the reaction, apart catalyser from reaction liquor by centrifugal machine till delimination in quiet placing, the above is rough output, the below is admixture of glycerol and carbinol. Distil the of above to gain bio-diesel oil and to gain the pure glycerin in the same way. The distilled carbinol can be used again and again. The invention has many advantages, for example, its raw material can be rebirth, its craft is easy and only need normal equipment. Even treat the used oil, the whole process is easier compared with the method in solid ac and alk catalyzing, besides, the process will not produce foul water so it is environmental. Every plant of the bio-diesel accords with standards compared with foreign similar competitive grade and the main plants are close to its of 0# (GB252-1994, superior product)diesel of China.
Description
(1) technical field
The present invention relates to green, field of renewable energy technology, be meant that specifically a kind of solid acid, base catalysis prepare method of bio-diesel oil.
(2) background technology
Diesel oil occupies higher share as a kind of important refining of petroleum product in various countries' fuel structure, become important power fuel.Along with the quickening of vehicle diesel oil trend in the world wide, the demand of following diesel oil can be more and more big, and the raising of exhausted day by day and people's environmental consciousness of petroleum resources, people begin to pay close attention to oil-fired substitute.Biofuel is to be the renewable energy source of raw material production with plant or animal grease, can be used as fine petroleum diesel surrogate.China is a large agricultural country, and agricultural resource is anxious to be waited to develop.Produce the selling market that thing diesel oil is maximum next life with Vegetable oil lipoprotein, so both adjusted the farm crop economic structure, improved peasant's income simultaneously again.This Study on Technology is not only benefited the nation and the people, and has realistic meaning.
Biofuel is a fatty acid methyl ester, is by the preparation of homogeneous catalysis ester-interchange method at present mostly, adopts liquid acid or liquid alkali catalyst, is generally NaOH, the KOH or the vitriol oil.If adopt the liquid alkali as a catalyst, stock oil and methyl alcohol must strictly dewater, otherwise easily form milk, and the free acid in the stock oil has very big infringement to the activity of basic catalyst.Also there is the people under the condition that liquid acid catalyst exists, to prepare biofuel, CN 1382762A adopts sulfuric acid or Phenylsulfonic acid to make catalyzer, CN 1412278A adopts sulfuric acid to make catalyzer, though liquid acid catalyst does not have particular requirement to the moisture and the free acid content of stock oil, but liquid acid has corrodibility, makes it very high to equipment requirements, and reaction end back methyl alcohol is difficult to separate with by-product glycerin, the last handling process complexity rises cost.In addition, adopt liquid acid or alkali, in last handling process, can discharge large amount of sewage, cause environmental pollution as catalyzer.Therefore, how to find a kind of appropriate catalyst, both reduced cost, simplify technical process, can reach the purpose of environmental protection again, become the focus that people pay close attention to.
(3) summary of the invention
The objective of the invention is to, propose a kind of employing solid acid, base catalysis prepares method of bio-diesel oil, it is complicated as the aftertreatment that catalyzer brings to have solved traditional employing liquid acid or liquid base, problems such as contaminate environment.
Technology of the present invention is as follows: under the condition of solid acid or solid base catalyst existence, low-carbon alcohol is mixed with vegetables oil, stir, heating makes it that transesterification reaction take place, and after reacting completely, with whizzer catalyst separating is gone out.With reaction mixture sat, two-layer about being divided into, the upper strata is a coarse products, is a series of Fatty acid methyl esters (biofuel) and the mixture that is dissolved in small amount of methanol wherein, and lower floor is glycerine and the mixed solution that remains methyl alcohol.To get biofuel behind the thick ester water-bath distillation in upper strata, get purified glycerine behind lower floor's water-bath distillation.The methyl alcohol that steams can also drop in the reaction cycle and reuse.
Processing condition relevant in the above-mentioned technology are as follows:
Catalyst levels accounts for the 2%-10% of stock oil weight;
Alcohol oil mole proportioning 3: 1-20: 1;
Transesterification reaction temperature 45-120 ℃;
3-15 hour transesterification reaction time.
Advantage of the present invention is:
1, the productive rate that adopts present method to prepare biofuel can reach more than 99%, and every performance index of product reach the standard of external like product substantially, and is close with the main performance index of China 0# diesel oil (GB252-1994, top grade product).
2, raw material sources are extensive, and are renewable; Technical process is simple, mild condition; Last handling process is simplified greatly; Whole reparation technology does not have any waste water, waste gas, and waste liquid produces, non-environmental-pollution.
3, byproduct glycerine is easy to separate and purifies, and reacts remaining methyl alcohol and can be recycled, and has avoided because byproduct is difficult to separate the huge waste that causes with methyl alcohol.
(4) embodiment
Embodiment one:
Raw material: soybean oil, methyl alcohol, zirconium sulfate.
(density is 0.92g/cm with the 80ml soybean oil
3) and 20ml methyl alcohol (density is 0.792g/cm
3) put into three mouthfuls of round-bottomed flasks of 250ml, stir, add 2.2 grams, 100 purpose zirconium sulfates, be heated to 65 ℃, react after 6 hours, stop to stir and heating.Earlier reaction solution is moved in the concentrator bowl zirconium sulfate is separated, pour into then in the separating funnel, leave standstill, be divided into two-layer up and down.
Behind upper strata water-bath distillation for removing methanol, promptly get biofuel 81.05 grams, productive rate can reach 99%, after residue methyl alcohol steams in the lower floor, gets 7.50 gram glycerine, and theoretical glycerine output is 7.57 grams, and the productive rate of calculating thus also is 99%, and is consistent with top conclusion.
With the biofuel product that makes with efficient liquid phase chromatographic analysis (chromatographic column VD-ODS (150L * 4.6), 25 ℃, 0.8ml/min, methyl alcohol for the solvent that loses shape, to inject volume be 5 microlitres), differentiate and find, triglyceride level, diester and monoesters have not existed in product, have been reformed completely into Fatty acid methyl ester and glycerine.Every performance index of the resulting biofuel of scale-up and 0# diesel oil (GB252-1994, top grade product) performance is compared as follows:
| Performance relatively | Density (15 ℃) g/cm 3 | Viscosity (40 ℃) mm 2/s | Flash-point | Sulphur content w% | Cetane value w% | Condensation point ℃ | Boiling range ℃ |
| 0# diesel oil | -- | ????3.0-8.0 | ??＞65 | ??≤0.2 | ??＞45 | ????0 | ????355 |
| Self-control diesel oil | 0.881 | ????4.75 | ＞85 (remaining silent) | ??0.0148 | ??47 | ????0 | ????350 |
Can find out that from last table the main performance index of its main performance index of homemade biofuel and China 0# diesel oil (GB252-1994, top grade product) is close.
Embodiment two:
Raw material: discarded edible oil, methyl alcohol, SO
4 2-/ ZrO
2
Earlier abendoned oil is purified: be heated to 50 ℃, the Tai-Ace S 150 of dropping 1% stirs centrifugally after 30 minutes, removes wherein colloid and impurity.Waste oil and the 21.38 gram methyl alcohol got after 72.80 grams purify are put into three mouthfuls of round-bottomed flasks of 250ml, stir, and add 2.9 gram 80-100 purpose SO
4 2-/ ZrO
2, be heated to 75 ℃, react after 8 hours, stop to stir and heating.Earlier reaction solution is moved in the concentrator bowl SO
4 2-/ ZrO
2Separate, pour into then in the separating funnel, leave standstill, be divided into two-layer up and down.With the upper strata water-bath distillation, remove methyl alcohol, decoloured 40 minutes down at 105 ℃, promptly get biofuel 72.90 grams, productive rate is 90%.
With the biofuel product that makes with efficient liquid phase chromatographic analysis (chromatographic column VD-ODS (150L * 4.6), 25 ℃, 0.8ml/min, methyl alcohol for the solvent that loses shape, to inject volume be 5 microlitres), differentiate and find, glycerin fatty acid ester and a large amount of free fatty acidies have been converted to a series of Fatty acid methyl esters, be biofuel, its every performance index are identical with embodiment one.
Embodiment three:
Raw material: soybean oil, methyl alcohol, zinc oxide
(density is 0.92g/cm with the 80ml soybean oil
3) and 20ml methyl alcohol (density is 0.792g/cm
3) put into three mouthfuls of round-bottomed flasks of 250ml, stir, add 2.2 gram 80-100 purpose zinc oxide, be heated to 65 ℃, react after 6 hours, stop to stir and heating.Earlier reaction solution is moved in the concentrator bowl zinc oxide is separated, pour into then in the separating funnel, leave standstill, be divided into two-layer up and down.
Behind upper strata water-bath distillation for removing methanol, promptly get biofuel 80.23 grams, productive rate can reach 98%, after residue methyl alcohol steams in the lower floor, gets 7.42 gram glycerine, and theoretical glycerine output is 7.57 grams, and the productive rate of calculating thus also is 98%, and is consistent with top conclusion.
The biofuel product that makes with efficient liquid phase chromatographic analysis (chromatographic column VD-ODS (150L * 4.6), 25 ℃, 0.8ml/min, methyl alcohol for the solvent that loses shape, to inject volume be 5 microlitres), is differentiated and found that product is a series of Fatty acid methyl esters.Its every performance index are identical with embodiment one.
Claims (7)
1, a kind of solid acid, base catalysis prepare method of bio-diesel oil, it is characterized in that: under the condition of solid acid or solid base catalyst existence, low-carbon alcohol is mixed with vegetables oil, continue to stir also heating, make it that transesterification reaction take place, reaction is isolated catalyzer with whizzer, the standing and reacting mixture after finishing, be divided into two-layer up and down, the upper strata is a coarse products, and lower floor is the mixed solution of glycerine and residue methyl alcohol, the methyl alcohol distillation of the upper and lower is removed promptly get biofuel and glycerine respectively.
2, solid acid according to claim 1, base catalysis prepare method of bio-diesel oil, and it is characterized in that: the solid acid catalyst that is adopted is: ZrSO
4, SO
4 2-/ ZrO
2, H-ZSM-5 type molecular sieve; Solid base catalyst is: zinc oxide, Mg-Al composite oxide catalysts, ETS-10 type molecular sieve.
3, solid acid according to claim 1, base catalysis prepare method of bio-diesel oil, it is characterized in that: the solid catalyst of adding is the 2%-10% of stock oil weight.
4, solid acid according to claim 1, base catalysis prepare method of bio-diesel oil, it is characterized in that: the optimum molar proportioning of methyl alcohol and soybean oil is 3: 1-20: 1.
5, solid acid according to claim 1, base catalysis prepare method of bio-diesel oil, it is characterized in that: transesterification reaction is carried out under 45-120 ℃, and the reaction times is 3-15 hour.
6, solid acid according to claim 1, base catalysis prepare method of bio-diesel oil, it is characterized in that: will get biofuel after the thick ester distillation in upper strata, and get purified glycerine after lower floor's distillation, the methyl alcohol that steams can be recycled.
7, solid acid according to claim 1, base catalysis prepare method of bio-diesel oil, it is characterized in that: described vegetables oil is soybean oil, genetically engineered soybean oil, rapeseed oil, transgenosis rapeseed oil, Viscotrol C, plam oil, peanut oil, sunflower seed oil, discarded edible oil; Described low-carbon alcohol is a methyl alcohol, ethanol, or the mixture of the two.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2004100382924A CN1580190A (en) | 2004-05-21 | 2004-05-21 | Method for preparing biodiesel by solid acid-base catalyst |
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|---|---|---|---|
| CNA2004100382924A CN1580190A (en) | 2004-05-21 | 2004-05-21 | Method for preparing biodiesel by solid acid-base catalyst |
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| CNA2004100382924A Pending CN1580190A (en) | 2004-05-21 | 2004-05-21 | Method for preparing biodiesel by solid acid-base catalyst |
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Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006128381A1 (en) * | 2005-06-03 | 2006-12-07 | Tsinghua University | Method for preparing 1,3-propanediol by using glycerine as the by-product of the biological diesel oil |
| CN100335594C (en) * | 2005-02-24 | 2007-09-05 | 浙江工业大学 | Method for preparing biological diesel oil |
| CN100341981C (en) * | 2006-02-27 | 2007-10-10 | 天津理工大学 | Technological process of preparing biological diesel oil continuously |
| CN100344732C (en) * | 2005-07-06 | 2007-10-24 | 中国科学院山西煤炭化学研究所 | Method of making biodiesel oil by subcritical methanol phase solid acid alkali catalytic oil fat ester exchange |
| CN100355860C (en) * | 2005-11-07 | 2007-12-19 | 清华大学 | Process for preparing bio- diesel oil by two-step catalysis of acid-containing fat |
| CN100357022C (en) * | 2005-03-23 | 2007-12-26 | 中国石油化工股份有限公司 | Load type calcium oxide catalyst, its preparation method and uses |
| CN100375780C (en) * | 2005-07-15 | 2008-03-19 | 清华大学 | Production of biological diesel oil with solid alkali |
| CN100415373C (en) * | 2006-10-30 | 2008-09-03 | 河南金龙工程技术有限公司 | Biodiesel oil methyl esterizing composite catalyst |
| CN100448946C (en) * | 2006-07-10 | 2009-01-07 | 中国科学院广州能源研究所 | Method for conitinuously producing biological diesel oil using solid acid catalyst and piston flow reactor |
| CN100503786C (en) * | 2006-06-02 | 2009-06-24 | 中国农业科学院油料作物研究所 | Method for preparing biological diesel oil using nano solid acid or alkali catalyst |
| CN100545240C (en) * | 2007-03-09 | 2009-09-30 | 厦门大学 | A kind of solid acid and solid alkali two-step catalysis method production method of bio-diesel oil utilized |
| CN101608131A (en) * | 2008-06-20 | 2009-12-23 | 华东理工大学 | A kind of biodiesel oil preparing process of no byproduct glycerol |
| CN100584925C (en) * | 2005-10-28 | 2010-01-27 | 原玉明 | Integral production method of bio-diesel oil and high protein feed |
| CN101230309B (en) * | 2008-01-11 | 2010-04-07 | 四川大学 | Method for preparing biodiesel by lowering value of high acid palm oil |
| CN101705155A (en) * | 2009-11-07 | 2010-05-12 | 青岛福瑞斯生物能源科技开发有限公司 | Method for industrially preparing biological diesel by waste grease |
| CN1900224B (en) * | 2005-06-15 | 2010-05-12 | 中国石油化工股份有限公司 | Process for preparing biological diesel oil |
| CN101067090B (en) * | 2007-06-08 | 2010-05-19 | 西北大学 | Solid catalysis for preparing biodiesel oil |
| CN101130163B (en) * | 2007-08-14 | 2010-05-19 | 西北农林科技大学 | Load type flyash solid base catalyst for producing biological diesel oil and method of producing the same |
| CN101067091B (en) * | 2007-06-08 | 2010-05-26 | 清华大学 | Solid catalysis process of preparing biodiesel oil continuously with high acid value material |
| CN101993784A (en) * | 2010-12-01 | 2011-03-30 | 沈阳工业大学 | Method for preparing biodiesel from hogwash oil catalyzed by solid super acid |
| CN1891787B (en) * | 2005-07-07 | 2011-04-06 | 南昌大学 | Production technology for preparing biodiesel by solid magnetic catalyst |
| CN102071109A (en) * | 2011-01-15 | 2011-05-25 | 青岛福瑞斯生物能源科技开发有限公司 | Method for decoloring biodiesel prepared from illegal cooking oil |
| CN101126029B (en) * | 2006-08-15 | 2011-08-17 | 广西师范大学 | Technique for preparing biological diesel oil by microwave catalyzing and film separating method |
| CN104560226A (en) * | 2014-11-04 | 2015-04-29 | 华文蔚 | Preparation method of biodiesel |
-
2004
- 2004-05-21 CN CNA2004100382924A patent/CN1580190A/en active Pending
Cited By (25)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100335594C (en) * | 2005-02-24 | 2007-09-05 | 浙江工业大学 | Method for preparing biological diesel oil |
| CN100357022C (en) * | 2005-03-23 | 2007-12-26 | 中国石油化工股份有限公司 | Load type calcium oxide catalyst, its preparation method and uses |
| WO2006128381A1 (en) * | 2005-06-03 | 2006-12-07 | Tsinghua University | Method for preparing 1,3-propanediol by using glycerine as the by-product of the biological diesel oil |
| CN1900224B (en) * | 2005-06-15 | 2010-05-12 | 中国石油化工股份有限公司 | Process for preparing biological diesel oil |
| CN100344732C (en) * | 2005-07-06 | 2007-10-24 | 中国科学院山西煤炭化学研究所 | Method of making biodiesel oil by subcritical methanol phase solid acid alkali catalytic oil fat ester exchange |
| CN1891787B (en) * | 2005-07-07 | 2011-04-06 | 南昌大学 | Production technology for preparing biodiesel by solid magnetic catalyst |
| CN100375780C (en) * | 2005-07-15 | 2008-03-19 | 清华大学 | Production of biological diesel oil with solid alkali |
| CN100584925C (en) * | 2005-10-28 | 2010-01-27 | 原玉明 | Integral production method of bio-diesel oil and high protein feed |
| CN100355860C (en) * | 2005-11-07 | 2007-12-19 | 清华大学 | Process for preparing bio- diesel oil by two-step catalysis of acid-containing fat |
| CN100341981C (en) * | 2006-02-27 | 2007-10-10 | 天津理工大学 | Technological process of preparing biological diesel oil continuously |
| CN100503786C (en) * | 2006-06-02 | 2009-06-24 | 中国农业科学院油料作物研究所 | Method for preparing biological diesel oil using nano solid acid or alkali catalyst |
| CN100448946C (en) * | 2006-07-10 | 2009-01-07 | 中国科学院广州能源研究所 | Method for conitinuously producing biological diesel oil using solid acid catalyst and piston flow reactor |
| CN101126029B (en) * | 2006-08-15 | 2011-08-17 | 广西师范大学 | Technique for preparing biological diesel oil by microwave catalyzing and film separating method |
| CN100415373C (en) * | 2006-10-30 | 2008-09-03 | 河南金龙工程技术有限公司 | Biodiesel oil methyl esterizing composite catalyst |
| CN100545240C (en) * | 2007-03-09 | 2009-09-30 | 厦门大学 | A kind of solid acid and solid alkali two-step catalysis method production method of bio-diesel oil utilized |
| CN101067090B (en) * | 2007-06-08 | 2010-05-19 | 西北大学 | Solid catalysis for preparing biodiesel oil |
| CN101067091B (en) * | 2007-06-08 | 2010-05-26 | 清华大学 | Solid catalysis process of preparing biodiesel oil continuously with high acid value material |
| CN101130163B (en) * | 2007-08-14 | 2010-05-19 | 西北农林科技大学 | Load type flyash solid base catalyst for producing biological diesel oil and method of producing the same |
| CN101230309B (en) * | 2008-01-11 | 2010-04-07 | 四川大学 | Method for preparing biodiesel by lowering value of high acid palm oil |
| CN101608131A (en) * | 2008-06-20 | 2009-12-23 | 华东理工大学 | A kind of biodiesel oil preparing process of no byproduct glycerol |
| CN101705155A (en) * | 2009-11-07 | 2010-05-12 | 青岛福瑞斯生物能源科技开发有限公司 | Method for industrially preparing biological diesel by waste grease |
| CN101993784A (en) * | 2010-12-01 | 2011-03-30 | 沈阳工业大学 | Method for preparing biodiesel from hogwash oil catalyzed by solid super acid |
| CN102071109A (en) * | 2011-01-15 | 2011-05-25 | 青岛福瑞斯生物能源科技开发有限公司 | Method for decoloring biodiesel prepared from illegal cooking oil |
| CN102071109B (en) * | 2011-01-15 | 2013-05-01 | 青岛福瑞斯生物能源科技开发有限公司 | Method for decoloring biodiesel prepared from illegal cooking oil |
| CN104560226A (en) * | 2014-11-04 | 2015-04-29 | 华文蔚 | Preparation method of biodiesel |
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